Acetic Acid → 2,6-Difluoro-3-methoxyphenol
反応式
[F:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[C:4]([F:10])[C:3]=1B(O)O.C(O)(=[O:16])C.OO>O1CCCC1>[F:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[C:4]([F:10])[C:3]=1[OH:16]参加物
5
実験手順
To a solution of 2,6-difluoro-3-methoxy-phenylboronic acid (10.0 g, 0.053 mol) in tetrahydrofuran (160 mL) was added glacial acetic acid (60 mL). The resulting mixture was cooled to 0° C. before hydrogen peroxide (50% aqueous solution, 8 mL) was added. The resulting mixture was allowed to come to room temperature and stirred for 120 h. The mixture was evaporated and the residue was dissolved in ethyl acetate, washed with hydrochloric acid (0.5N), water and brine. The organic phase was dried, filtered and evaporated which afforded 2,6-difluoro-3-methoxy-phenol (7.50 g, 88%) as a pale brown solid.
後処理
- additionwas added
- customto come to room temperature
- customThe mixture was evaporated
- dissolutionthe residue was dissolved in ethyl acetate
- washwashed with hydrochloric acid (0.5N), water and brine
- customThe organic phase was dried
- filtrationfiltered
- customevaporated which
出典と根拠
- ORDレコード
- ord-e127866cdd7a4ef6a9febf1bd21ca98f
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741327B2
反応ノート
読み込み中…